CN110690446A - Preparation method of carbon-coated ferroferric oxide for iron-nickel battery - Google Patents
Preparation method of carbon-coated ferroferric oxide for iron-nickel battery Download PDFInfo
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- CN110690446A CN110690446A CN201910934205.XA CN201910934205A CN110690446A CN 110690446 A CN110690446 A CN 110690446A CN 201910934205 A CN201910934205 A CN 201910934205A CN 110690446 A CN110690446 A CN 110690446A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/30—Nickel accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery, which comprises the following steps: (1) mixing Fe3O4Mixing with certain amount of conductive graphite, and ball milling for certain period; (2) calcining the ball-milled substance in an argon atmosphere for a period of time to obtain a cathode precursor; (3) uniformly mixing the negative electrode precursor with a conductive agent and an additive, and then adding a binder and deionized water to prepare slurry; (4) uniformly coating the slurry on foamed nickel, and drying in a vacuum drying oven to obtain a pole piece; (5) rolling and spot-welding the pole piece with a tab; (6) and (4) placing the pole piece obtained in the step (5) in a diaphragm, assembling the pole piece and the positive electrode into a battery, and then adding alkaline electrolyte to obtain the iron-nickel battery. By the preparation method of the carbon-coated ferroferric oxide for the iron-nickel battery, the iron-nickel battery can be preparedPreparation of Nano Fe3O4the/C composite material increases the electrical conductivity of the pole piece, reduces polarization, improves the discharge specific capacity of the iron-nickel battery, has large specific surface area and improves the large-current discharge performance. And the method is simple and easy to operate, so that the production cost is reduced.
Description
Technical Field
The invention relates to the technical field of iron-nickel batteries, and in particular relates to a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery.
Background
An iron-nickel battery is an alkaline storage battery in which a positive electrode active material is mainly made of nickel and a negative electrode active material is mainly made of iron. Iron-nickel batteries have been developed for over a hundred years, but because of large volume, heavy weight, complex maintenance and poor low-temperature performance, the field of vision of people is gradually faded out due to weak environmental awareness of people at that time. In recent years, the iron-nickel battery returns to the public vision due to the enhanced public environmental protection awareness, and attracts the attention of scholars at home and abroad.
In recent years, scholars at home and abroad improve the electrochemical performance of the iron-nickel battery by various methods, particularly a preparation method of a negative electrode material. Currently synthesized Fe3O4The chemical methods mainly include coprecipitation method, neutralization precipitation method, sol-gel method, precipitation oxidation method, electrochemical method, microemulsion method, hydrothermal method, hydrolysis method, polyol method, etc. However, the iron electrode still has some problems such as passivation phenomenon, gassing problem, etc. The commercial iron negative electrode has a low gram capacity, the gram capacity of the active substance can only reach 200mAh/g, and the specific energy is low, and although the preparation of the lithium ion negative electrode material is more researched, the lithium ion negative electrode material is different from the iron-nickel battery in working principle, so the preparation method of the lithium ion negative electrode material is not suitable for preparing the negative electrode material of the iron-nickel battery.
Therefore, it is urgently needed to explore a new preparation method for the cathode material of the iron-nickel battery to solve the above-mentioned deficiencies of the prior art.
Disclosure of Invention
The invention aims to provide a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery, which can be used for preparing nano-scale iron oxideRice Fe3O4the/C composite material increases the electrical conductivity of the pole piece, reduces polarization, improves the discharge specific capacity of the iron-nickel battery, has large specific surface area and improves the large-current discharge performance. And the method is simple and easy to operate, so that the production cost is reduced.
In order to achieve the aim, the invention provides a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery, which comprises the following steps:
(1) mixing Fe3O4Mixing with certain amount of conductive graphite, and ball milling for certain period;
(2) calcining the ball-milled substance in an argon atmosphere for a period of time to obtain a cathode precursor;
(3) uniformly mixing the negative electrode precursor with a conductive agent and an additive, and then adding a binder and deionized water to prepare slurry;
(4) uniformly coating the slurry on foamed nickel, and drying in a vacuum drying oven to obtain a pole piece;
(5) rolling and spot-welding the pole piece with a tab;
(6) and (4) placing the pole piece obtained in the step (5) in a diaphragm, assembling the pole piece and the positive electrode into a battery, and then adding alkaline electrolyte to obtain the iron-nickel battery.
Compared with the prior art, in the preparation method of the carbon-coated ferroferric oxide for the iron-nickel battery, Fe is utilized3O4Ball-milling the mixture after the mixture is even with conductive graphite, and calcining the mixture for a period of time in argon atmosphere to obtain a cathode precursor, thereby preparing the nanoscale Fe for the iron-nickel battery3O4Anode material, i.e. nano-Fe3O4the/C composite material can increase the electrical conductivity of the pole piece, reduce polarization, improve the discharge specific capacity of the iron-nickel battery, has large specific surface area and improves the large-current discharge performance. And the method is simple and easy to operate, so that the cost can be reduced. Further, nano Fe3O4The iron-nickel battery has excellent specific discharge capacity and high-current discharge performance by matching the/C composite material with the conductive agent, the additive and the binder.
Preferably, the assembly is carried out in a mode of two positive electrodes and one negative electrode.
Preferably, the conductive agent is at least two of graphite, nickel powder or iron powder, although the conductive effect of graphite is good, if the system is used for a long time, the graphite is oxidized, and the conductive performance is reduced, so that the service life of the iron-nickel battery is prolonged when the graphite is used together with the nickel powder or the iron powder.
Preferably, the additive is at least one of ferrous sulfide or bismuth trioxide.
Preferably, the binder is at least one of polytetrafluoroethylene and sodium carboxymethyl cellulose.
Preferably, the content of the conductive graphite is Fe3O45% -40%.
Preferably, the content of the conductive graphite is Fe3O410 percent of the total weight of the conductive graphite is Fe3O4When the content is 10%, the discharge specific capacity of the iron-nickel battery is better.
Preferably, in the step (6), the alkaline electrolyte is a mixed solution of potassium hydroxide and lithium hydroxide.
Preferably, the conductive agent is graphite, nickel powder and iron powder, the additive is ferrous sulfide and bismuth trioxide, the binder is polytetrafluoroethylene and sodium carboxymethylcellulose, the alkaline electrolyte is a mixed solution of potassium hydroxide and lithium hydroxide, and the conductive agent is matched with Fe by using the substances3O4The iron-nickel battery obtained by the/C composite material has excellent electrochemical performance.
Preferably, in step (5), the rolling thickness is 0.5mm to 0.8mm, such as 0.5mm, 0.6mm, 0.7mm, 0.8 mm.
Wherein, in the step (1), the ball milling time is 5-36h, and the ball milling rotating speed is 300-.
Wherein, in the step (2), the heating rate of the calcination is 3-5 ℃/min, the calcination temperature is 400-800 ℃, and the calcination time is 4-8 h.
Wherein, in the step (4), the temperature of the vacuum drying oven is 60-90 ℃, and the drying time is 3-8 h.
And (4) standing for a period of time after the iron-nickel battery is obtained in the step (6), and then testing, wherein the standing time is 4-8 h.
The invention will become more apparent from the following description when taken in conjunction with the accompanying drawings, which illustrate embodiments of the invention.
Drawings
Fig. 1 is an SEM image of the negative electrode precursor in example 1.
FIG. 2 is a comparison graph of specific discharge capacity of carbon-coated ferroferric oxide with different contents.
FIG. 3 shows Fe with 10% of ferroferric oxide in conductive graphite3O4C and Fe without conductive graphite coating3O4Comparative graph of specific discharge capacity of (a).
Fig. 4 is a graph comparing specific discharge capacities of iron-nickel batteries with different additives.
Detailed Description
Example 1:
a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery comprises the following steps:
(1) 200g of Fe3O4Uniformly mixing the graphite powder with 20g of conductive graphite, and placing the mixture on a roller horizontal ball mill for ball milling for 6 hours;
(2) and placing the ball-milled substance in a corundum crucible, and calcining for 2h at 700 ℃ in an argon atmosphere to obtain a cathode precursor.
(3) Uniformly mixing 100g of the negative electrode precursor with 2g of graphite, 4g of iron powder, 1g of nickel powder, 1.5g of ferrous sulfide and 2g of bismuth trioxide, then adding 20g of sodium carboxymethylcellulose and 4g of polytetrafluoroethylene aqueous solution, and then adding 20g of deionized water to prepare slurry;
(4) uniformly coating the slurry on foamed nickel, and drying in a vacuum drying oven at 60 ℃ for 6h to obtain a pole piece;
(5) rolling the pole piece to 0.55mm, and spot-welding the pole lug;
(6) and (5) placing the pole piece obtained in the step (5) in a diaphragm, assembling the pole piece and a positive pole into a battery, adding a mixed solution of potassium hydroxide and lithium hydroxide to obtain the iron-nickel battery, standing for 6 hours, and testing the charge and discharge performance of the iron-nickel battery.
Example 2:
a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery comprises the following steps:
(1) 200g of Fe3O4Mixing with 10g of conductive graphite uniformly, and placing on a roller horizontal ball mill for ball milling for 6 hours;
(2) and placing the ball-milled substance in a corundum crucible, and calcining for 2h at 700 ℃ in an argon atmosphere to obtain a cathode precursor.
(3) Uniformly mixing 100g of the negative electrode precursor with 2g of graphite, 4g of iron powder, 1g of nickel powder, 1.5g of ferrous sulfide and 2g of bismuth trioxide, then adding 20g of sodium carboxymethylcellulose and 4g of polytetrafluoroethylene aqueous solution, and then adding 20g of deionized water to prepare slurry;
(4) uniformly coating the slurry on foamed nickel, and drying in a vacuum drying oven at 60 ℃ for 6h to obtain a pole piece;
(5) rolling the pole piece to 0.55mm, and spot-welding the pole lug;
(6) and (5) placing the pole piece obtained in the step (5) in a diaphragm, assembling the pole piece and a positive pole into a battery, adding a mixed solution of potassium hydroxide and lithium hydroxide to obtain the iron-nickel battery, standing for 6 hours, and testing the charge and discharge performance of the iron-nickel battery.
Example 3:
a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery comprises the following steps:
(1) 200g of Fe3O4Uniformly mixing the graphite powder with 30g of conductive graphite, and placing the mixture on a roller horizontal ball mill for ball milling for 6 hours;
(2) and placing the ball-milled substance in a corundum crucible, and calcining for 2h at 700 ℃ in an argon atmosphere to obtain a cathode precursor.
(3) Uniformly mixing 100g of the negative electrode precursor with 2g of graphite, 4g of iron powder, 1g of nickel powder, 1.5g of ferrous sulfide and 2g of bismuth trioxide, then adding 20g of sodium carboxymethylcellulose and 4g of polytetrafluoroethylene aqueous solution, and then adding 20g of deionized water to prepare slurry;
(4) uniformly coating the slurry on foamed nickel, and drying in a vacuum drying oven at 60 ℃ for 6h to obtain a pole piece;
(5) rolling the pole piece to 0.55mm, and spot-welding the pole lug;
(6) and (5) placing the pole piece obtained in the step (5) in a diaphragm, assembling the pole piece and a positive pole into a battery, adding a mixed solution of potassium hydroxide and lithium hydroxide to obtain the iron-nickel battery, standing for 6 hours, and testing the charge and discharge performance of the iron-nickel battery.
Example 4:
a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery comprises the following steps:
(1) 200g of Fe3O4Uniformly mixing the graphite powder with 20g of conductive graphite, and placing the mixture on a roller horizontal ball mill for ball milling for 6 hours;
(2) and placing the ball-milled substance in a corundum crucible, and calcining for 2h at 700 ℃ in an argon atmosphere to obtain a cathode precursor.
(3) Uniformly mixing 100g of the negative electrode precursor, 2g of graphite, 4g of iron powder, 1g of nickel powder and 1.5g of ferrous sulfide, then adding 4g of polytetrafluoroethylene aqueous solution, and then adding 20g of deionized water to prepare slurry;
(4) uniformly coating the slurry on foamed nickel, and drying in a vacuum drying oven at 60 ℃ for 6h to obtain a pole piece;
(5) rolling the pole piece to 0.55mm, and spot-welding the pole lug;
(6) and (5) placing the pole piece obtained in the step (5) in a diaphragm, assembling the pole piece and a positive pole into a battery, adding a mixed solution of potassium hydroxide and lithium hydroxide to obtain the iron-nickel battery, standing for 6 hours, and testing the charge and discharge performance of the iron-nickel battery.
Example 5:
a preparation method of carbon-coated ferroferric oxide for an iron-nickel battery comprises the following steps:
(1) 200g of Fe3O4Uniformly mixing the graphite powder with 20g of conductive graphite, and placing the mixture on a roller horizontal ball mill for ball milling for 6 hours;
(2) and placing the ball-milled substance in a corundum crucible, and calcining for 2h at 700 ℃ in an argon atmosphere to obtain a cathode precursor.
(3) Uniformly mixing 100g of the negative electrode precursor with 2g of graphite, 4g of iron powder, 1g of nickel powder, 1.5g of ferrous sulfide and 2g of bismuth trioxide, then adding 4g of polytetrafluoroethylene aqueous solution, and then adding 20g of deionized water to prepare slurry;
(4) uniformly coating the slurry on foamed nickel, and drying in a vacuum drying oven at 60 ℃ for 6h to obtain a pole piece;
(5) rolling the pole piece to 0.55mm, and spot-welding the pole lug;
(6) and (5) placing the pole piece obtained in the step (5) in a diaphragm, assembling the pole piece and a positive pole into a battery, adding a mixed solution of potassium hydroxide and lithium hydroxide to obtain the iron-nickel battery, standing for 6 hours, and testing the charge and discharge performance of the iron-nickel battery.
Comparative example 1
Comparative example No Fe3O4The treatment is carried out by directly using 100g of Fe3O4After being uniformly mixed with 2g of graphite, 4g of iron powder, 1g of nickel powder, 1.5g of ferrous sulfide and 2g of bismuth trioxide, 20g of sodium carboxymethylcellulose and 4g of polytetrafluoroethylene aqueous solution are added, and 20g of deionized water is added to prepare the slurry. The remaining procedure was the same as in example 3.
The negative electrode precursor obtained in example 1 was subjected to SEM test, and the result is shown in fig. 1, and as is clear from fig. 1, Fe3O4the/C composite material is in a nanometer level, and the specific surface area is large.
Electrochemical test measurements of the iron-nickel batteries obtained in examples 1 to 3 and comparative example 1 are shown in FIGS. 2 to 3, and it can be seen from FIG. 2 that the content of the conductive graphite is Fe3O4When the content is 10%, the discharge specific capacity of the iron-nickel battery is better. As can be seen from FIG. 3, Fe coated with conductive graphite3O4As a negative electrode, the discharge specific capacity of the iron-nickel battery is far superior to that of unpaired Fe3O4And (4) performing treatment on the iron-nickel battery.
As shown in fig. 4, the results of electrochemical test measurements on the iron-nickel batteries obtained in examples 4 to 5 are shown in fig. 4, and it is understood from fig. 4 that the specific discharge capacity of the iron-nickel battery is greatly improved when bismuth trioxide is added.
The present invention has been described in connection with the preferred embodiments, but the present invention is not limited to the embodiments disclosed above, and is intended to cover various modifications, equivalent combinations, which are made in accordance with the spirit of the present invention.
Claims (10)
1. A preparation method of carbon-coated ferroferric oxide for an iron-nickel battery is characterized by comprising the following steps:
(1) mixing Fe3O4Mixing with certain amount of conductive graphite, and ball milling for certain period;
(2) calcining the ball-milled substance in an argon atmosphere for a period of time to obtain a cathode precursor;
(3) uniformly mixing the negative electrode precursor with a conductive agent and an additive, and then adding a binder and deionized water to prepare slurry;
(4) uniformly coating the slurry on foamed nickel, and drying in a vacuum drying oven to obtain a pole piece;
(5) rolling and spot-welding the pole piece with a tab;
(6) and (4) placing the pole piece obtained in the step (5) in a diaphragm, assembling the pole piece and the positive electrode into a battery, and then adding alkaline electrolyte to obtain the iron-nickel battery.
2. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 1, wherein the assembly is performed in a mode of two positive electrodes and one negative electrode.
3. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 1, wherein the conductive agent is at least two of graphite, nickel powder or iron powder.
4. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 1, wherein the additive is at least one of ferrous sulfide or bismuth trioxide.
5. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 1, wherein the binder is at least one of polytetrafluoroethylene and sodium carboxymethylcellulose.
6. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 1, wherein the content of the conductive graphite is Fe3O45% -40%.
7. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 6, wherein the content of the conductive graphite is Fe3O410% of the total.
8. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 1, wherein in the step (6), the alkaline electrolyte is a mixed solution of potassium hydroxide and lithium hydroxide.
9. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 1, wherein the conductive agent is graphite, nickel powder and iron powder, the additive is ferrous sulfide and bismuth trioxide, the binder is polytetrafluoroethylene and sodium carboxymethylcellulose, and the alkaline electrolyte is a mixed solution of potassium hydroxide and lithium hydroxide.
10. The method for preparing carbon-coated ferroferric oxide for an iron-nickel battery according to claim 1, wherein in the step (5), the rolling thickness is 0.5mm to 0.8 mm.
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| CN111146431A (en) * | 2020-02-11 | 2020-05-12 | 河南创力新能源科技股份有限公司 | Iron-nickel battery cathode composite material and preparation method thereof |
| CN111146408A (en) * | 2020-02-11 | 2020-05-12 | 河南创力新能源科技股份有限公司 | Preparation method of iron-nickel battery cathode |
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